반응 #657275

ord-476249cbcfe6473cb8c58188d6000e04

반응 방정식

CC1CCCC(C)N1CC(=O)NCC(=O)O
[2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid
O=C1CCC(=O)N1O
N-Hydroxysuccinimide
C(=NC1CCCCC1)=NC1CCCCC1
N,N′-Dicyclohexyl-carbodiimide
CC1CCCC(C)N1CC(=O)NCC(=O)ON1C(=O)CCC1=O
[2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The solution was filtered
  2. 2
    기타the filtrate was evaporated in vacuo to dryness
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in 50 mL dichloromethane
  4. 4
    workup.ADDITIONtreated with charcoal
  5. 5
    여과After filtration
  6. 6
    기타the solution was evaporated in vacuo to dryness
  7. 7
    기타the product was recrystallised from ethyl acetate

실험 절차

4.54 g (20 mMol) [2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid (30) were added to 2.30 g (20 mMol) N-Hydroxysuccinimide and 4.12 g (20 mMol) N,N′-Dicyclohexyl-carbodiimide dissolved in 150 ml dichloromethane. The reaction mixture was stirred for 16 h at room temperature. The solution was filtered and the filtrate was evaporated in vacuo to dryness. The residue was dissolved in 50 mL dichloromethane and treated with charcoal. After filtration, the solution was evaporated in vacuo to dryness and the product was recrystallised from ethyl acetate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09023656B2uspto-grants-2015_05